홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Isopropanol → HCID 178431911, 화합물

HRID 1637640
노트
인쇄 미리보기

반응식

HRID 1637640 반응식
ClC[C:3]1[C:8]([CH3:9])=[C:7]([S:10][CH2:11][CH2:12][CH2:13][S:14][C:15]2[CH:16]=[CH:17][C:18]3[N:19]([C:21]([N+:24]([O-:26])=[O:25])=[CH:22][N:23]=3)[N:20]=2)[CH:6]=[CH:5][N:4]=1.[SH:27][C:28]1[N:32]([C:33]2[CH:38]=[CH:37][C:36]([OH:39])=[CH:35][CH:34]=2)[N:31]=[N:30][N:29]=1.[CH:40](O)(C)C>>[CH3:9][C:8]1[C:3]([SH:27]([CH3:40])[C:28]2[N:32]([C:33]3[CH:34]=[CH:35][C:36]([OH:39])=[CH:37][CH:38]=3)[N:31]=[N:30][N:29]=2)=[N:4][CH:5]=[CH:6][C:7]=1[S:10][CH2:11][CH2:12][CH2:13][S:14][C:15]1[CH:16]=[CH:17][C:18]2[N:19]([C:21]([N+:24]([O-:26])=[O:25])=[CH:22][N:23]=2)[N:20]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 3776IsopropanolHCID 187993836-[3-(2-Chloromethyl-3-methylpyridin-4-ylsulfanyl)propylsulfanyl]-3-nitroimidazo[1,2-b]pyridazineHCID 178516236HCID 178516236, 화합물

생성물 1

HCID 178431911HCID 178431911, 화합물수율 75%

반응 조건

온도
0 °C

실험 절차

0.61 g (1.5 mmol) of 6-[3-(2-chloromethyl-3-methylpyridin-4-ylsulfanyl)propylsulfanyl]-3-nitroimidazo[1,2-b]pyridazine and 0.30 g (1.5 mmol) of 4-(5-mercaptotetrazol-1-yl)phenol in 30 ml of isopropanol are heated under reflux for 2 h under a nitrogen atmosphere. The mixture is then concentrated. The residue is taken up in 30 ml of water, adjusted to pH 9 using 2N sodium hydroxide solution and extracted with 4×30 ml of dichloromethane. The organic extracts are washed with water, dried over magnesium sulfate and concentrated. The residue is taken up in 200 ml of hot acetonitrile, clarified with active carbon, filtered, concentrated to a volume of 50 ml and cooled to 0° C. The precipitate is filtered off, washed with acetonitrile and dried. 0.64 g (75%) of the title compound is isolated as a pale beige solid. M.p. 92° C. (dec.).

후처리

  1. temperatureunder reflux for 2 h under a nitrogen atmosphere
  2. concentrationThe mixture is then concentrated
  3. extractionextracted with 4×30 ml of dichloromethane
  4. washThe organic extracts are washed with water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated
  7. filtrationfiltered
  8. concentrationconcentrated to a volume of 50 ml
  9. filtrationThe precipitate is filtered off
  10. washwashed with acetonitrile
  11. customdried

출처 및 근거

ORD 기록
ord-c8a6881333fc46e58f1e6233c4727024
출처 데이터셋
uspto-grants-2000_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06043242

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트